#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/47/2224749.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2224749
loop_
_publ_author_name
'Huang, Xihe'
'Liu, Zhongqian'
'Huang, Changcang'
'Wang, Yubo'
_publ_section_title
;
 catena-Poly[zinc(II)-μ₃-{hydrogen
 [1-hydroxy-2-(3-pyridinio)ethane-1,1-diyl]diphosphonato}]
;
_journal_coeditor_code           RZ2390
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m59
_journal_page_last               m60
_journal_paper_doi               10.1107/S1600536809052702
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Zn (C7 H9 N O7 P2)]'
_chemical_formula_moiety         'C7 H9 N O7 P2 Zn'
_chemical_formula_sum            'C7 H9 N O7 P2 Zn'
_chemical_formula_weight         346.46
_chemical_name_systematic
;
catena-Poly[zinc(II)-μ₃-{hydrogen
[1-hydroxy-2-(3-pyridinio)ethane-1,1-diyl]diphosphonato}]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.21(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.609(3)
_cell_length_b                   5.4809(11)
_cell_length_c                   14.818(3)
_cell_measurement_reflns_used    3898
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.6491
_cell_measurement_theta_min      3.0520
_cell_volume                     1084.2(4)
_computing_cell_refinement       'CrystalClear (Rigaku, 2002)'
_computing_data_collection       'CrystalClear (Rigaku, 2002)'
_computing_data_reduction        'CrystalClear (Rigaku, 2002)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL/PC (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku Mercury CCD area-detector'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_sigmaI/netI    0.0193
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8250
_diffrn_reflns_theta_full        27.69
_diffrn_reflns_theta_max         27.69
_diffrn_reflns_theta_min         3.72
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.587
_exptl_absorpt_correction_T_max  0.8197
_exptl_absorpt_correction_T_min  0.6257
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(RAPID-AUTO; Rigaku, 1998)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.123
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.324
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2519
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0258
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0218P)²+1.6938P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0607
_refine_ls_wR_factor_ref         0.0612
_reflns_number_gt                2473
_reflns_number_total             2519
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            rz2390.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2224749
_cod_database_fobs_code          2224749
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn Zn1 0.412237(17) 0.25347(4) 0.425508(16) 0.01698(8) Uani d . 1 . .
P P1 0.29107(4) 0.76285(9) 0.37901(3) 0.01399(11) Uani d . 1 . .
P P2 0.36304(4) 0.92659(9) 0.57727(3) 0.01507(11) Uani d . 1 . .
O O1 0.32521(11) 1.0088(3) 0.34936(9) 0.0191(3) Uani d . 1 . .
O O2 0.36616(12) 0.5657(3) 0.37738(10) 0.0234(3) Uani d . 1 . .
O O3 0.18869(11) 0.6951(3) 0.31670(10) 0.0253(3) Uani d . 1 . .
H H3 0.1983 0.6398 0.2677 0.038 Uiso d R 1 . .
O O4 0.37845(11) 1.1832(3) 0.54302(10) 0.0201(3) Uani d . 1 . .
O O5 0.44985(11) 0.7562(3) 0.57500(12) 0.0259(3) Uani d . 1 . .
O O6 0.33324(11) 0.9324(3) 0.66920(9) 0.0234(3) Uani d . 1 . .
O O7 0.23742(11) 0.5508(3) 0.52251(10) 0.0211(3) Uani d . 1 . .
H H7 0.2870 0.4642 0.5252 0.032 Uiso d R 1 . .
N N1 0.10323(14) 1.1013(4) 0.71483(12) 0.0263(4) Uani d . 1 . .
H H1 0.1173 1.2169 0.7545 0.032 Uiso calc R 1 . .
C C1 0.25880(14) 0.7897(4) 0.49374(13) 0.0149(4) Uani d . 1 . .
C C2 0.16165(15) 0.9394(4) 0.48646(13) 0.0190(4) Uani d . 1 . .
H H2A 0.1753 1.1076 0.4727 0.023 Uiso calc R 1 . .
H H2B 0.1121 0.8769 0.4357 0.023 Uiso calc R 1 . .
C C3 0.11892(14) 0.9324(4) 0.57271(13) 0.0179(4) Uani d . 1 . .
C C4 0.06000(17) 0.7409(4) 0.59111(16) 0.0243(5) Uani d . 1 . .
H H4A 0.0452 0.6148 0.5487 0.029 Uiso calc R 1 . .
C C5 0.02268(19) 0.7328(4) 0.67077(17) 0.0295(5) Uani d . 1 . .
H H5A -0.0182 0.6046 0.6819 0.035 Uiso calc R 1 . .
C C6 0.04682(18) 0.9168(5) 0.73327(16) 0.0301(5) Uani d . 1 . .
H H6A 0.0239 0.9131 0.7884 0.036 Uiso calc R 1 . .
C C7 0.13858(16) 1.1135(4) 0.63744(14) 0.0219(4) Uani d . 1 . .
H H7A 0.1772 1.2468 0.6271 0.026 Uiso calc R 1 . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O5 Zn1 O2 3_666 . 106.21(7) ?
O5 Zn1 O4 3_666 1_545 114.36(7) ?
O2 Zn1 O4 . 1_545 113.44(6) ?
O5 Zn1 O1 3_666 1_545 117.63(7) ?
O2 Zn1 O1 . 1_545 106.02(7) ?
O4 Zn1 O1 1_545 1_545 99.08(6) ?
O2 P1 O1 . . 112.93(9) ?
O2 P1 O3 . . 110.75(9) ?
O1 P1 O3 . . 109.18(9) ?
O2 P1 C1 . . 111.10(9) ?
O1 P1 C1 . . 109.71(9) ?
O3 P1 C1 . . 102.68(9) ?
O6 P2 O5 . . 112.64(10) ?
O6 P2 O4 . . 111.29(9) ?
O5 P2 O4 . . 113.84(9) ?
O6 P2 C1 . . 108.04(9) ?
O5 P2 C1 . . 103.62(9) ?
O4 P2 C1 . . 106.78(9) ?
P1 O1 Zn1 . 1_565 128.06(8) ?
P1 O2 Zn1 . . 144.97(10) ?
P1 O3 H3 . . 109.5 ?
P2 O4 Zn1 . 1_565 123.97(9) ?
P2 O5 Zn1 . 3_666 143.43(10) ?
C1 O7 H7 . . 109.4 ?
C7 N1 C6 . . 122.4(2) ?
C7 N1 H1 . . 118.8 ?
C6 N1 H1 . . 118.8 ?
O7 C1 C2 . . 106.72(16) ?
O7 C1 P1 . . 107.57(13) ?
C2 C1 P1 . . 109.45(13) ?
O7 C1 P2 . . 110.31(13) ?
C2 C1 P2 . . 111.50(14) ?
P1 C1 P2 . . 111.12(10) ?
C3 C2 C1 . . 113.26(16) ?
C3 C2 H2A . . 108.9 ?
C1 C2 H2A . . 108.9 ?
C3 C2 H2B . . 108.9 ?
C1 C2 H2B . . 108.9 ?
H2A C2 H2B . . 107.7 ?
C7 C3 C4 . . 117.04(19) ?
C7 C3 C2 . . 121.41(19) ?
C4 C3 C2 . . 121.53(19) ?
C5 C4 C3 . . 121.4(2) ?
C5 C4 H4A . . 119.3 ?
C3 C4 H4A . . 119.3 ?
C6 C5 C4 . . 118.6(2) ?
C6 C5 H5A . . 120.7 ?
C4 C5 H5A . . 120.7 ?
N1 C6 C5 . . 119.7(2) ?
N1 C6 H6A . . 120.2 ?
C5 C6 H6A . . 120.2 ?
N1 C7 C3 . . 120.9(2) ?
N1 C7 H7A . . 119.6 ?
C3 C7 H7A . . 119.6 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Zn1 O5 3_666 1.8791(16) y
Zn1 O2 . 1.9121(15) y
Zn1 O4 1_545 1.9243(15) y
Zn1 O1 1_545 1.9888(15) y
P1 O2 . 1.4907(15) y
P1 O1 . 1.5182(15) y
P1 O3 . 1.5594(16) y
P1 C1 . 1.843(2) y
P2 O6 . 1.4953(15) y
P2 O5 . 1.5115(16) y
P2 O4 . 1.5236(15) y
P2 C1 . 1.851(2) y
O1 Zn1 1_565 1.9888(15) ?
O3 H3 . 0.8200 ?
O4 Zn1 1_565 1.9243(15) ?
O5 Zn1 3_666 1.8791(16) ?
O7 C1 . 1.424(2) ?
O7 H7 . 0.8201 ?
N1 C7 . 1.329(3) ?
N1 C6 . 1.330(3) ?
N1 H1 . 0.8600 ?
C1 C2 . 1.542(3) ?
C2 C3 . 1.504(3) ?
C2 H2A . 0.9700 ?
C2 H2B . 0.9700 ?
C3 C7 . 1.370(3) ?
C3 C4 . 1.380(3) ?
C4 C5 . 1.373(3) ?
C4 H4A . 0.9300 ?
C5 C6 . 1.366(3) ?
C5 H5A . 0.9300 ?
C6 H6A . 0.9300 ?
C7 H7A . 0.9300 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O3 H3 O1 2_545 0.82 1.85 2.637(2) 161.1
N1 H1 O6 2_556 0.86 1.68 2.533(2) 169.6
O7 H7 O4 1_545 0.82 1.97 2.758(2) 162.5
